CN109020513A - 一种纳米氧化铜掺杂的氧化铝-氧化锆长效抗菌生物陶瓷的制备方法 - Google Patents
一种纳米氧化铜掺杂的氧化铝-氧化锆长效抗菌生物陶瓷的制备方法 Download PDFInfo
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Abstract
本发明属于抗菌植入体材料的技术领域,公开了一种掺杂纳米氧化铜的氧化铝‑氧化锆长效抗菌生物陶瓷的制备方法。所述制备方法为:将球磨介质,α‑Al2O3,ZrO2(HfO2)和Y2O3的混合物,TiO2,SiO2,SrO,CuO(其中CuO含量为0~1%)置于球磨装置中进行球磨,搅拌干燥,造粒,压片初成型,冷等静压成型,煅烧,得到掺杂纳米氧化铜的氧化铝‑氧化锆长效抗菌生物陶瓷。采用平板计数法对制备的陶瓷球头进行了抗菌实验,得到了很好的效果。采用本发明的方法制备的掺杂纳米氧化铜的氧化铝‑氧化锆长效抗菌生物陶瓷植入体具有较好的抗菌效果和力学性能,具有节约能源的优点。
Description
技术领域
本发明属于抗菌材料领域,特别涉及一种掺杂纳米氧化铜的氧化铝-氧化锆抗菌生物陶瓷的制备方法。
背景技术
氧化铝陶瓷属于生物惰性陶瓷,植入到人体后不会引起周围组织和全身明显的化学和生物排斥反应。高纯氧化铝陶瓷是最早临床应用的陶瓷,具有良好的力学性能、生物相容性,优良的抗腐蚀性和耐磨性,但是氧化铝陶瓷材料存在断裂韧性非常低的问题,极大地限制了该陶瓷材料的使用。因此采用耐磨抗冲击的氧化锆增韧氧化铝陶瓷,氧化锆可增强生物陶瓷材料的断裂韧性和断裂强度。
氧化铝-氧化锆陶瓷作为生物植入材料植入人体的过程中容易面临两个重要的问题,分别是植入松动和细菌感染,这也是氧化铝-氧化锆陶瓷植入失败的两个重要原因。其中细菌感染这一问题对植入过程造成了很大困扰,一但细菌生物膜和植入体结合,将导致材料植入失败,甚至会导致严重的细菌感染和创口溃疡。因此,构建能够阻止或减少细菌黏附及增殖的生物陶瓷材料的应用具有重大意义。
发明内容
针对现有技术的不足,本发明的目的是提供一种掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的制备方法。
本发明的目的是通过以下技术方案来实现的:
一种掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的制备方法,包括以下步骤:
(1)称取以下原料(按质量分数计):50%~90%α-Al2O3,7.1%~49.97%ZrO2(HfO2)和Y2O3的混合物,0.1%~0.7%TiO2,0.1%~0.7%SiO2,0.1%~0.5%SrO,0%~1%CuO;
(2)将步骤(1)所称量的陶瓷粉料放到60℃烘干,烘干后的陶瓷粉体加入行星式球磨机中,配成料浆,并球磨6~12h,球磨的转速为200~450rpm;
(3)将步骤(2)所制得的浆料在70℃下加热搅拌干燥,进行研磨、过筛处理,过筛的目数为60~100目;
(4)将步骤(3)所制得的研磨粉体加入1%~8%粘接剂,再次研磨过筛;
(5)将步骤(4)所制得的陶瓷粉体静置陈化24h,采用手扳式压机初压成坯体,之后采用冷等静压成型再次压制,压力为180~250MPa;
(6)将步骤(5)所制得的球体坯体烘干至含水率为1%~2%,将烘干的球体坯体煅烧;
(7)将步骤(6)煅烧后的样品打磨抛光后干燥保存。
优选的,步骤(1)所述的CuO的一次粒径d为30~200nm。
优选的,步骤(2)所述的料浆是由陶瓷粉体材料和无水乙醇配成,固含量
为50%。
优选的,步骤(3)所述干燥后陶瓷粉体的含水率小于0.5%。
优选的,步骤(4)所述的粘接剂是由聚乙烯醇和水以(80%~95%):(5%~20%)
的比例混合而成。
优选的,步骤(6)所述煅烧温度为1450~1650℃,保温时间为1~4h。
与现有技术相比,本发明具有以下有益效果:
(1)采用本发明方法制备的掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的抗菌率达到95%以上。所用的纳米氧化铜具有高效持久抗菌作用,一方面可以采用溶出的锌离子Cu2+抗菌,其机制为纳米氧化铜接触细菌破坏细胞膜导致细胞内容物的溶出,从而使细菌丧失其生物学活性等而完成杀菌过程。另一方面纳米氧化铜产生的活性氧抗菌,其机制为通过电子自旋共振测定发现,纳米氧化铜可激发产生活性羟基,而活性羟基可进一步通过多步反应产生H2O2等其他活性氧基团。活性氧最为显著的特点就是可以造成氧化压力,可以造成DNA、细胞膜、蛋白质的损伤,甚至可以引起细胞死亡;
(2)采用本发明方法制备的掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷具有更好的力学性能,采用的纳米氧化铜对微米结构的陶瓷材料进行填充,可以提高陶瓷材料的力学性能;
(3)采用本发明方法制备的掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷降低了烧结温度,节约了资源,而且有利于陶瓷致密度的提高。
附图说明
图1是一种掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷制备流程图。
具体实施方式
下面结合具体实施例对本发明作进一步地具体详细描述,但本发明的实施方式不限于此,对于未特别注明的工艺参数,可参照常规技术进行。
以下实施方案中α-Al2O3原料一次粒径d50为0.1μm,纯度为99.99%;ZrO2(HfO2)和Y2O3的混合物原料一次粒径d50为0.399μm,纯度为99.9%,CuO为市面购买的粒径为40nm。
实施例1
一种掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的制备方法,包括以下步骤:
(1)称取以下原料(按质量分数算):90%α-Al2O3,9.25%ZrO2(HfO2)和Y2O3的混合物,0.25%TiO2,0.25%SiO2,0.25%SrO;
(2)将步骤(1)所称量的陶瓷粉料放到60℃烘干,烘干后的陶瓷粉体加入行星式球磨机中,配成料浆,并球磨8h,球磨的转速为200~450rpm;
(3)将步骤(2)所制得的浆料在70℃下加热搅拌干燥,进行研磨、过筛处理,过筛的目数为80目;
(4)将步骤(3)所制得的研磨粉体加入5%粘接剂,再次研磨过筛;
(5)将步骤(4)所制得的陶瓷粉体静置陈化24h,采用手扳式压机初压成坯体,之后采用冷等静压成型再次压制,压力为200MPa;
(6)将步骤(5)所制得的球体坯体烘干至含水率为1%,将烘干的球体坯体煅烧;
(7)将步骤(6)煅烧后的样品打磨抛光后干燥保存。
步骤(1)所述的CuO的一次粒径d为40nm;
步骤(2)所述的料浆是由陶瓷粉体材料和无水乙醇配成,固含量为50%;
步骤(3)所述的干燥后陶瓷粉体的含水率小于0.5%;
步骤(4)所述的粘接剂是由聚乙烯醇和水以80%:20%的比例混合而成;
步骤(6)所述的煅烧温度为1650℃,保温时间为2h;
实施例2
一种掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的制备方法,包括以下步骤:
(1)称取以下原料(按质量分数算):90%α-Al2O3,8.95%ZrO2(HfO2)和Y2O3的混合物,0.25%TiO2,0.25%SiO2,0.25%SrO,0.3%CuO;
(2)将步骤(1)所称量的陶瓷粉料放到60℃烘干,烘干后的陶瓷粉体加入行星式球磨机中,配成料浆,并球磨8h,球磨的转速为200~450rpm;
(3)将步骤(2)所制得的浆料在70℃下加热搅拌干燥,进行研磨、过筛处理,过筛的目数为80目;
(4)将步骤(3)所制得的研磨粉体加入5%粘接剂,再次研磨过筛;
(5)将步骤(4)所制得的陶瓷粉体静置陈化24h,采用手扳式压机初压成坯体,之后采用冷等静压成型再次压制,压力为200MPa;
(6)将步骤(5)所制得的球体坯体烘干至含水率为1%,将烘干的球体坯体煅烧;
(7)将步骤(6)煅烧后的样品打磨抛光后干燥保存。
步骤(1)所述的CuO的一次粒径d为40nm;
步骤(2)所述的料浆是由陶瓷粉体材料和无水乙醇配成,固含量为50%;
步骤(3)干燥后陶瓷粉体的含水率小于0.5%;
步骤(4)所述的粘接剂是由聚乙烯醇和水以80%:20%的比例混合而成;
步骤(6)中所述煅烧温度为1550℃,保温时间为2h;
实施例3
一种掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的制备方法,包括以下步骤:
(1)称取以下原料(按质量分数算):60%α-Al2O3,38.5%ZrO2(HfO2)和Y2O3的混合物,0.4%TiO2,0.4%SiO2,0.4%SrO,0.3%CuO;
(2)将步骤(1)所称量的陶瓷粉料放到60℃烘干,烘干后的陶瓷粉体加入行星式球磨机中,配成料浆,并球磨8h,球磨的转速为200~450rpm;
(3)将步骤(2)所制得的浆料在70℃下加热搅拌干燥,进行研磨、过筛处理,过筛的目数为80目;
(4)将步骤(3)所制得的研磨粉体加入5%粘接剂,再次研磨过筛;
(5)将步骤(4)所制得的陶瓷粉体静置陈化24h,采用手扳式压机初压成坯体,之后采用冷等静压成型再次压制,压力为200MPa;
(6)将步骤(5)所制得的球体坯体烘干至含水率为1%,将烘干的球体坯体煅烧;
(7)将步骤(6)煅烧后的样品打磨抛光后干燥保存。
步骤(1)所述的CuO的一次粒径d为40nm;
步骤(2)所述的料浆是由陶瓷粉体材料和无水乙醇配成,固含量为50%;
步骤(3)干燥后陶瓷粉体的含水率小于0.5%;
步骤(4)所述的粘接剂是由聚乙烯醇和水以80%:20%的比例混合而成;
步骤(6)所述煅烧温度为1550℃,保温时间为2h;
实施例4
一种掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的制备方法,包括以下步骤:
(1)称取以下原料(按质量分数算):50%α-Al2O3,48.5%ZrO2(HfO2)和Y2O3的混合物,0.4%TiO2,0.4%SiO2,0.4%SrO,0.3%CuO;
(2)将步骤(1)所称量的陶瓷粉料放到60℃烘干,烘干后的陶瓷粉体加入行星式球磨机中,配成料浆,并球磨8h,球磨的转速为200~450rpm;
(3)将步骤(2)所制得的浆料在70℃下加热搅拌干燥,进行研磨、过筛处理,过筛的目数为80目;
(4)将步骤(3)所制得的研磨粉体加入5%粘接剂,再次研磨过筛;
(5)将步骤(4)所制得的陶瓷粉体静置陈化24h,采用手扳式压机初压成坯体,之后采用冷等静压成型再次压制,压力为200MPa;
(6)将步骤(5)所制得的球体坯体烘干至含水率为1%,将烘干的球体坯体煅烧;
(7)将步骤(6)煅烧后的样品打磨抛光后干燥保存。
步骤(1)所述的CuO的一次粒径d为40nm;
步骤(2)所述的料浆是由陶瓷粉体材料和无水乙醇配成,固含量为50%;
步骤(3)干燥后陶瓷粉体的含水率小于0.5%;
步骤(4)所述的粘接剂是由聚乙烯醇和水以80%:20%的比例混合而成;
步骤(6)所述煅烧温度为1550℃,保温时间为2h;
为了验证实施例的抗菌效果,具体的抗菌实现方案及检测结果如下:
(1)液体培养基的配置及灭菌
采用的是营养肉汤,其配比为肉汤18g:蒸馏水或者去离子水1L,搅拌加热煮沸至完全溶解,121℃高温灭菌
(2)固体培养基的配置及灭菌
配比是:营养琼脂33g:蒸馏水或者去离子水1L,搅拌加热煮沸至完全溶解,121℃高温灭菌后,冷却至温度为50℃-70℃,固体培养基的高度是培养皿高度的1/2-2/3。
(3)纯化和培养细菌
取20μl冻存的细菌稀释1000倍后吸取20μl涂在(2)中琼脂板上,培养12h后用灭菌枪头挑选的单个的菌落放到盛有5ml液体培养基的摇菌管中培养8-12h;
(4)材料与细菌共培养
a.以OD值=0.1为标准计算实验中合适的菌液浓度并配置;
b.将a中得到的菌液加入到放有氧化铝-氧化锆陶瓷材料(实施例1~4所制备陶瓷材料)的孔板中共培养2h和12h;
(5)涂板
当材料和细菌共培养2h时将(4b)中的菌液稀释100倍后利用涂布棒均匀的涂在(2)中冷却成型的琼脂板后放于37℃生化培养箱中培养12h;
当材料和细菌共培养12h时将(4b)中的菌液稀释100倍后利用涂布棒均匀的涂在(2)中冷却成型的琼脂板后放于37℃生化培养箱中培养12h。
(6)菌落计数
经过培养,由每个单细胞生长繁殖而形成肉眼可见的菌落,统计菌落数,根据其稀释倍数和取样接种量即可换算出样品中的含菌数。选菌落数在30-300之间的培养皿进行菌落计数,然后对比各个材料菌落数,说明材料的抗菌性能。实施例1~4所制备的掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的抗菌性能测试结果表1所示。
表1实施案例制备的陶瓷材料的抗菌性能
为了验证实施例的力学性能效果,具体的力学性能测试方案及检测结果如下:
将所测试陶瓷材料打磨抛光后,使用相对面夹角为136°的正四棱锥金刚石压头以9.807N(HV1)的负荷作用于材料表面,保持规定时间后,测量压痕对角线长度,再按公式来计算硬度的大小。实施例1~4所制备的掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的力学性能性能测试结果表2所示。
表2实施案例制备的陶瓷材料的力学性能
显然,本发明的上述实施例仅仅是为清楚地说明本发明所作的举例,而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明权利要求的保护范围之内。
Claims (6)
1.一种掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的制备方法,其特征在于,包括以下步骤:
S1.称取以下陶瓷原料(按质量分数计):50%~90% α-Al2O3,7.1%~49.97% ZrO2(HfO2)和Y2O3的混合物,0.1%~0.7%TiO2,0.1%~0.7% SiO2,0.1%~0.5% SrO,0%~1%CuO;
S2.将步骤S1所称量的陶瓷粉料放到60℃烘干,烘干后的陶瓷粉体加入行星式球磨机中,配成料浆,并球磨6~12h,球磨的转速为200~450rpm;
S3.将步骤S2所制得的浆料在70℃下加热搅拌干燥,进行研磨、过筛处理,过筛的目数为60~100目;
S4.将步骤S3所制得的研磨粉体加入1%~8%粘接剂,再次研磨过筛;
S5.将步骤S4所制得的陶瓷粉体静置陈化24h,采用手扳式压机初压成坯体,之后采用冷等静压成型再次压制,压力为180~250MPa;
S6.将步骤S5所制得的球体坯体烘干至含水率为1%~2%,将烘干的球体坯体煅烧;
S7.将步骤S6煅烧后的样品打磨抛光后干燥保存。
2.根据权利要求1所述掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的制备方法,其特征在于,步骤S1所述的CuO的一次粒径d为30~200nm。
3.根据权利要求1所述所述掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的制备方法,其特征在于,步骤S2所述的料浆是由陶瓷粉体材料和无水乙醇配成,固含量为50%。
4.根据权利要求1所述掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的制备方法,其特征在于,步骤S3所述干燥后陶瓷粉体的含水率小于0.5%。
5.根据权利要求1所述掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的制备方法,其特征在于,步骤S4所述的粘接剂是由聚乙烯醇和水以(80%~95%):(5%~20%)的比例混合而成。
6.根据权利要求1所述掺杂纳米氧化铜的氧化铝-氧化锆长效抗菌的生物陶瓷的制备方法,其特征在于,步骤S6所述煅烧温度为1450~1650℃,保温时间为1~4h。
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Application publication date: 20181218 |
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